scholarly journals Beiträge zur Chemie des Phosphors, 96 [1] Darstellung und 31P-Kernresonanzspektrum von isotopen-substituiertem Trilithium-heptaphosphid, 6Li3P7 / Contributions to the Chemistry of Phosphorus, 96 [1] Preparation and 31P NMR Spectrum of Isotopicly Substituted Trilithiumheptaphosphide, 6Li3P7

1980 ◽  
Vol 35 (5) ◽  
pp. 517-521 ◽  
Author(s):  
Marianne Baudler ◽  
Thomas Pontzen ◽  
Josef Hahn ◽  
Hans Ternberger ◽  
Wolfgang Faber
Keyword(s):  
Room Temperature ◽  
31P Nmr ◽  
Chemical Shifts ◽  
Exchange Process ◽  
Complete Analysis ◽  
Ionic Character ◽  
Line Broadening ◽  
Threefold Axis ◽  
Nmr Spectrum ◽  
Li Isotope

Abstract The P7-skeleton of trilithiumheptaphosphide, Li3P7 (1), was proved to possess the earlier reported tricyclic structure [2] by complete analysis of the 31P NMR spectrum of 6Li3P7 observed at - 60 °C. The 6Li isotopic substitution was carried out to avoid the line broadening caused by the large quadrupole moment of the 7Li isotope. The unambiguous elucidation of the Li3P7 structure confirmed that the exchange process which causes all P atoms to become equivalent above room temperature is analogous to that in bullvalene. A comparison of the chemical shifts with those of (Me3Si)3P7 leads to the result that the P7-skeleton in Li3P7 is noticeably compressed along its threefold axis, thus indicating a predominant ionic character.

Beiträge zur Chemie des Phosphors, 147 [1] 31P-Kernresonanzspektrum und Struktur von Hexaethyl-octaphosphan(6), P8Et6 / Contributions to the Chemistry of Phosphorus, 147 [1] 31P NMR Spectrum and Structure of Hexaethyloctaphosphane(6), P8Et6

1984 ◽  
Vol 39 (12) ◽  
pp. 1671-1675 ◽  
Author(s):  
Marianne Bäudler ◽  
Eberhard Därr ◽  
Gerhard Binsch ◽  
David S. Stephenson
Keyword(s):  
31P Nmr ◽  
Chemical Shifts ◽  
Coupling Constants ◽  
Complete Analysis ◽  
Nmr Spectrum ◽  
H Nmr ◽  
Configuration And Conformation

Hexaethyloctaphosphane(6) (1) was proven to possess the structure of a 2,3,4,6,7,8-hexaethylbicyclo[3.3.0]octaphosphane by a complete analysis of its 31P {1H } NMR spectrum. The chemical shifts and coupling constants yielded inform ation about the configuration and conformation of 1.

scholarly journals Beiträge zur Chemie des Phosphors, 132 [1]. 31P-Kernresonanzspektrum und Struktur von Trimethylheptaphosphan(3), P7Me3 / Contributions to the Chemistry of Phosphorus, 132 [1]. 31P NMR Spectrum and Structure of Trimethylheptaphosphane(3), P7Me3

1983 ◽  
Vol 38 (8) ◽  
pp. 955-960 ◽  
Author(s):  
Marianne Bäudler ◽  
Thomas Pontzen
Keyword(s):  
31P Nmr ◽  
Chemical Shifts ◽  
Experimental Spectrum ◽  
Complete Analysis ◽  
Methyl Groups ◽  
Nmr Spectrum ◽  
H Nmr

Trimethylheptaphosphane(3) (1) was proved to possess the earlier reported structure of a 3,5,7-triorganotrieyclo[2.2.1.02,6] heptaphosphane [3] by complete analysis of its 31P{1H} NMR spectrum. The experimental spectrum can be simulated very satisfactorily by the superposition of the spectra of two isomers P7Me3sym and P7Me3 asym, differing from each other in the orientation of the methyl groups. A comparison of the chemical shifts with those of (Me3Si)3P7 and Li3P7 leads to a detailed information about the geometry of the P7-skeleton in both isomers of 1.

29Si, 13C and 31P NMR spectra of silicon-substituted ω-diphenylphosphinoalkyl silanes, (CH3)3-n(OC2H5)nSi(CH2)mP(C6H5)2

1982 ◽  
Vol 47 (3) ◽  
pp. 793-801 ◽  
Author(s):  
Jan Schraml ◽  
Martin Čapka ◽  
Harald Jancke
Keyword(s):  
Nmr Spectra ◽  
31P Nmr ◽  
Chemical Shifts ◽  
Additivity Rule ◽  
Ethoxy Group ◽  
Spectral Parameters ◽  
Nmr Spectrum ◽  
Nmr Parameters ◽  
13C And 31P Nmr ◽  
C Nmr

29Si, 13C, and 31P NMR spectra of a series of compounds of the structure (CH3)3-n(C2H5O)n.Si(CH2)mP(C6H5)2 (m = 1-6, n = )-3) are reported and assigned. Using monodeutero derivative of the compound with m = 3 and n = 0 an earlier assignment of 13C NMR spectrum is confirmed, but the assignment in the compounds with m = 4 is reversed. Introduction of ethoxy groups leads to violation of additivity rule for the 13C chemical shifts in the derivatives with m = 1. In all derivatives presence of one ethoxy group in the molecule has a profound effect on 31P chemical shift which is not changed by any further increase in the number of ethoxy groups in the molecule. The changes in 29Si chemical shifts follow the pattern known from other series of compounds. The observed trends in NMR parameters with changing n and m values can be explained by an interaction between phosphorus and oxygen atoms. Possible connections between the spectral parameters and catalysis employing the studied compounds are discussed.

scholarly journals 1H- and 31P-NMR Spectroscopy Study of Paramagnetic Lanthanide Coordination Compounds [LnL3 • Phen] (L = CCl3C(O)NP(O)(OCH3)2)

2019 ◽  
Vol 64 (9) ◽  
pp. 855
Author(s):  
V. A. Trush ◽  
O. O. Litsis ◽  
T. Yu. Sliva ◽  
Ya. O. Gumenyuk ◽  
V. M. Amirkhanov
Keyword(s):  
Nmr Spectroscopy ◽  
Coordination Sphere ◽  
Coordination Compounds ◽  
Room Temperature ◽  
31P Nmr ◽  
Chemical Shifts ◽  
31P Nmr Spectroscopy ◽  
Spectroscopy Study

A series of lanthanide coordination compounds with dimethyl-N-trichloroacetylamidophosphate CCl3C(O)N(H)P(O)(OCH3)2 (HL) [HL = CCl3C(O)N(H)P(O)(OCH3)2 is a ligand of the carbacylamidophosphate (CAPh) type], whose compositions are described by the formula [LnL3 · Phen], where Ln = La, Ce, Pr, Nd, Sm, Tb, Dy, Ho, and Er; L is the deprotonized form of HL; and Phen is 1,10-Phenantroline, has been synthesized. Acetonic solutions of HL and complexes synthesized on its basis are studied by means of 1H- and 31P-NMR spectroscopy at room temperature (298 K). Since the chemical shifts of 1H signals have the pseudocontactorigin, the isotropic shifts of 31P signals are managed to be decomposed into the contact and pseudocontact components. It is found that there are two series of complexes in the solution of [LnL3 · Phen] compounds with the same structure of the coordination sphere within each of the series Ln = (Ce, Pr, Nd, Sm) (series L1) and Ln = (Tb, Dy, Ho, Er) (series L2). The values of the constant of superfine interaction for those complexes are calculated: 0.18 MHz (series L1) and 0.13 MHz (series L2).

1H NMR, 31P NMR and Raman Study of CaHPO4 and SrHPO4

2005 ◽  
Vol 60 (1-2) ◽  
pp. 121-126 ◽  
Author(s):  
B. Louati ◽  
K. Guidara ◽  
M. Gargouri ◽  
M. Fourati
Keyword(s):  
1H Nmr ◽  
Nmr Spectra ◽  
Room Temperature ◽  
31P Nmr ◽  
Cross Polarization ◽  
Nmr Spectrum ◽  
H Nmr ◽  
Nmr Techniques ◽  
Raman Study

CaHPO4 and SrHPO4 were investigated using Raman, 1H NMR and 31P NMR techniques to study the environment of their PO3−4 tetrahedra and the percentage of mobile protons. 1H NMR spectra at room temperature suggest the presence of three types of protons, in agreement with RX investigation. The percentage of mobile protons in SrHPO4 is greater than in CaHPO4 because Sr2+ is bigger than Ca2+. 31P NMR spectra at room temperature show two lines in the spectrum of SrHPO4, revealing an equal environment of two sets of pairs of PO3− 4 . The 31P NMR spectrum of CaHPO4, however, exhibits three lines. This result was confirmed using a cross polarization (CP) sequence program. The first peak is attributed to the first set of pairs of P(1)O4 units and the two other ones to P(2)O4 and P(2)O4 units.

Dimethylhalonium-Ionen in Aluminiumhalogenid/Methylhalogenid-Lösungen / Dimethylhalonium-Ions in Aluminium Halide/Methyl Halide Solutions

1979 ◽  
Vol 34 (7) ◽  
pp. 896-899 ◽  
Author(s):  
Peter Brüggeller ◽  
Erwin Mayer
Keyword(s):  
Time Scale ◽  
Low Temperatures ◽  
Room Temperature ◽  
Chemical Shifts ◽  
Ion Concentration ◽  
Molar Ratio ◽  
Lower Field ◽  
Nmr Spectrum ◽  
H Nmr ◽  
Methyl Halide

Abstract Evidence for the formation of (CH3)2Br+ and (CH3)2I+ in CH3Br and CH3I solutions saturated with AlBr3 comes from the appearance of a second singlet in the 1H NMR spectrum. The (CH3)2Br+ ion is formed at -40 °C to about 5 mol%, the (CH3)2I+ ion at -12 °C with 50 mol% yield. At higher temperatures the concentration of the halonium ions decreases rapidly. The (CH3)2Br+ ion is not detectable at room temperature, the concentration of (CH3)2I+ decreases to about 30 mol%. Dilution of the saturated solutions with methyl halide also reduces the halonium ion concentration. An AlBr3/CH3Br solution with a molar ratio of 1:3 at -40 °C shows no sign of (CH3)2Br+ formation in the XH NMR spectrum. Both effects are best explained by formation of dimethylhalonium ions from the adduct CH3X-AIX3 and by dependence of adduct concentration on temperature and dilution. Exchange of (CH3)2Br+ and (CH3)2I+ with methyl halide is slow on the NMR time scale at low temperatures similar to the results in SbF5/SO2. The 1H NMR singlets of (CH3)2Br+ and (CH3)2I+ are shifted to lower field by 1.32 and 1.68 ppm in comparison with the chemical shifts in SbF5/SO2 solution

Beiträge zur Chemie des Phosphors, 161 [1] Kernresonanzspektren und Struktur von Heptaphosphan(3), P7H3 / Contributions to the Chemistry of Phosphorus, 161 [1] NMR Spectra and Structure of Heptaphosphane(3), P7H3

1985 ◽  
Vol 40 (11) ◽  
pp. 1424-1429 ◽  
Author(s):  
Marianne Bäudler ◽  
Renate Riekehof-Böhmer
Keyword(s):  
Nmr Spectra ◽  
Chemical Shifts ◽  
Spatial Arrangement ◽  
Complete Analysis ◽  
Hydrogen Atoms ◽  
Nmr Spectrum ◽  
H Nmr

Heptaphosphane(3) (1) is obtained pure by the reaction of (Me3Si)3P7 with methanol and has been characterized NMR spectroscopically (in nascent state). It turned out to be a mixture of two diastereomers P7H3sym and P7H3asym, which differ in the spatial arrangement of the hydrogen atoms. Both isomers were proven to possess the earlier reported structure of a tri-cyclo[2.2.1.02,6]heptaphosphane, which in the case of P7H3sym was ascertained by a complete analysis of its 31P{1H} NMR spectrum. As shown by the chemical shifts, the P7 cage in P7H3sym is clearly stretched compared with P7Me3sym and (Me3Si)3P7.

21,22-Disubstituted 18α,19βH-Ursane Derivatives with Oxabicyclooctane System in Ring E

1993 ◽  
Vol 58 (1) ◽  
pp. 173-190 ◽  
Author(s):  
Eva Klinotová ◽  
Jiří Klinot ◽  
Václav Křeček ◽  
Miloš Buděšínský ◽  
Bohumil Máca
Keyword(s):  
Spectral Data ◽  
Spin Systems ◽  
Coupling Constants ◽  
Complete Analysis ◽  
Nmr Spectrum ◽  
Proton Proton ◽  
H Nmr ◽  
Proton Coupling ◽  
C Nmr

Reaction of 3β-acetoxy-21,22-dioxo-18α,19βH-ursan-28,20β-olide (IIIa) and 20β,28-epoxy-21,22-dioxo-19α,19βH-ursan-3β-yl acetate (IIIb) with diazomethane afforded derivatives XII-XIV with spiroepoxide group in position 21 or 22, which were further converted into hydroxy derivatives XV and XVII. Ethylene ketals VIII-X were also prepared. In connection with the determination of position and configuration of the functional groups at C(21) and C(22), the 1H and 13C NMR spectral data of the prepared compounds are discussed. Complete analysis of two four-spin systems in the 1H NMR spectrum of bisethylenedioxy derivative Xb led to the proton-proton coupling constants from which the structure with two 1,4-dioxane rings condensed with ring E, and their conformation, was derived.

Temperature-induced structural phase transitions in RERhSn (RE = Y, Gd-Tm, Lu)

2021 ◽  
Vol 0 (0) ◽  
Author(s):  
Simon Engelbert ◽  
Rolf-Dieter Hoffmann ◽  
Jutta Kösters ◽  
Steffen Klenner ◽  
Rainer Pöttgen
Keyword(s):  
Rare Earth ◽  
Phase Transitions ◽  
Driving Force ◽  
Room Temperature ◽  
Structural Phase ◽  
Structural Phase Transitions ◽  
Line Broadening ◽  
X Ray Diffraction ◽  
Temperature Dependent ◽  
X Ray

Abstract The structures of the equiatomic stannides RERhSn with the smaller rare earth elements Y, Gd-Tm and Lu were reinvestigated on the basis of temperature-dependent single crystal X-ray diffraction data. GdRhSn crystallizes with the aristotype ZrNiAl at 293 and 90 K. For RE = Y, Tb, Ho and Er the HP-CeRuSn type (approximant with space group R3m) is already formed at room temperature, while DyRhSn adopts the HP-CeRuSn type below 280 K. TmRhSn and LuRhSn show incommensurate modulated variants with superspace groups P31m(1/3; 1/3; γ) 000 (No. 157.1.23.1) (γ = 3/8 for TmRhSn and γ = 2/5 for LuRhSn). The driving force for superstructure formation (modulation) is a strengthening of Rh–Sn bonding. The modulation is expressed in a 119Sn Mössbauer spectrum of DyRhSn at 78 K through line broadening.

X-Ray Diffraction Study of Hep Metals. I. Line Broadening in Polycrystalline Cd Powder

1974 ◽  
Vol 29 (12) ◽  
pp. 1771-1777 ◽  
Author(s):  
N. C. Haider ◽  
S. H. Hunter
Keyword(s):  
Room Temperature ◽  
Small Deformation ◽  
Correction Factors ◽  
Line Broadening ◽  
X Ray Diffraction ◽  
Fault Probability ◽  
Large Particle Size ◽  
X Ray ◽  
Melting Temperatures ◽  
Diffraction Patterns

Powder Cd of 99.999% purity was prepared at room temperature (25 °C) and x-ray diffraction patterns were obtained using CuKaα radiation with Ni-filter. The line broadening was analyzed after incorporating the appropriate correction factors. At room temperature Cd was found to have large particle size (653 A), small root mean square strain (.001), small deformation fault probability a (.003). and negligible growth fault probability β(0). Compared to other hep metals which have been studied earlier and which have higher melting temperatures, metal Cd is much less affected by mechanical deformation at room temperature.

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